Catalytically activated vacuum distillation system

ABSTRACT

A catalytically activated vacuum distillation system, several novel component parts of said system, a process for producing carbon based products and novel carbon black that is produced from such a system and process.

This application claims priority from U.S. Provisional UtilityApplication No. 60/681,701, filed on May 17, 2005.

The invention disclosed and claimed herein deals with a catalyticallyactivated vacuum distillation system, several novel component parts ofsaid system, a process for producing carbon based products and novelcarbon black that is produced from such a system and process.

BACKGROUND OF THE INVENTION

The published art is replete with examples of converting waste materialsinto useful hydrocarbon gases, liquids, and other carbon containingproducts. Early attempts at converting such materials to usefulhydrocarbon gases, liquids and other carbon containing products includedstraight pyrolysis of such wastes.

Later studies led to the use of catalysts to enhance the breakdown ofthe waste materials. These thermal and/or catalytic assisted thermalcracking techniques were carried out under high temperatures and/orpressures, often entailing the use of temperatures in excess of 1500° F.and pressures in excess of 2,000 psi during the process. Theseconditions necessitated heavy equipment, and sometimes specializedequipment, to deal with the high temperatures and high pressures.

One such process can be found in U.S. Pat. No. 5,414,169, that issued toTakahashi, et al. on May 9, 1995 wherein there is disclosed a method ofobtaining hydrocarbon oil from waste plastic material or waste rubbermaterial, comprising the steps of subjecting the waste plastic materialor a waste rubber material to thermal cracking so as to obtain athermally cracked product, then liquefying the thermally cracked productinto a liquefied product, and then causing a liquid phase crackingreaction of the liquefied product under the action of a catalyst on theliquefied product so as to produce a cracked product, and then coolingthe cracked product so as to obtain the hydrocarbon oil.

U.S. Pat. No. 5,744,668, that issued on Apr. 28, 1998 to Zhou, et al.,deals with a process of producing gasoline, diesel and carbon black withwaste rubber and/or waste plastics. The process comprises pyrolysis,purifying, catalytic cracking and fractionation, similar to the '169patent.

U.S. Pat. No. 6,270,630 that issued on Aug. 7, 2001 to Xing deals with aprocess and apparatus for producing hydrocarbons from residential trashor waste and/or organic waste materials, and deals primarily with theapparatus that is used for such process. The process requires that theorganic waste materials are treated by a two-step cracking process, atdifferent temperatures, with successive feeding and discharging.

There is disclosed in U.S. Pat. No. 6,653,517, that issued on Nov. 25,2003 to Bullock, a method and apparatus for converting both organic andinorganic materials into more desirable products by the breaking down ofthese materials into their stable molecular constituents and reformingthem into more desirable substances. The process involves the use of twochambers. Blended solid and fluid wastes are augured into the firstchamber and agitated, preferably by rotating the chamber so that thewaste tumbles over internal fins, while a heat gradient is applied. Theprocess is catalyzed and the patentees use other means of enhancing theprocess.

U.S. Pat. No. 6,833,486, that issued on Dec. 21, 2004 to Nichols, et al,deals with a low energy method of pyrolysis of hydrocarbon materialssuch as rubber. In the process, the hydrocarbon material is heated whilemaintaining a vacuum using a clay catalyst. However, the catalyst isadded to the feedstock of the process and is not put into the heatedreactor prior to the introduction of the feedstock to the reactor as inthe present invention.

A similar process can be found in U.S. Pat. No. 6,835,861, that issuedDec. 28, 2004 to Nichols, et al. in which the hydrocarbon materials isheated while maintaining a vacuum using a clay catalyst. This patent isa companion patent to the '486 patent. As in the '486 patent, theprocess requires that the hydrocarbon material and the catalyst becombined prior to feeding into the reaction chamber, and in column 4,line 65, to column 5, line 3, it is explained that the hydrocarbonmaterial is added to the reactor first, then the clay catalyst, and themixture is heated under vacuum conditions. In addition, at column 5,lines 28 to 30, it is disclosed that adding metals can be catalyzingcertain reactions a augments the process.

A second patent to Bullock is U.S. Pat. No. 6,653,517, that issued onNov. 25, 2003 that deals with a hydrocarbon conversion apparatus andmethod. The apparatus includes a pair of retort vessels in communicationwith each other, one of which has two chambers, one chamber containing afluidized bed of catalytic feed and abrasive materials and the other acrusher mill. The vessels include lifting and stirring elements fixed tothe interior walls to promote and help maintain a condition offluidization of bed materials during operation. This process operates atnegative pressure.

Finally, the patentees are aware of U.S. Pat. No. 6,210,562, that issuedon Apr. 3, 2001 to Xie, et al that deals with a process for productionof ethylene and propylene by catalytic pyrolysis of heavy hydrocarbons.A pillared interlayered clay molecular sieve and/or phosphorous andaluminum or magnesium or calcium modified high silica zeolites are usedas catalysts.

THE INVENTION

The invention disclosed and claimed herein deals with a catalyticallyactivated vacuum distillation system, several novel component parts ofsaid system, a process for producing carbon based products and novelcarbon black that is produced from such a system and process.

The catalytically activated vacuum distillation system comprises incombination (I) a feed hopper, wherein the feed hopper is capable ofcontaining water in it. There is a feed conveyor, the feed conveyorcomprising a first elongated hollow housing having a top side andcontained therein, a rotatable screw feeding mechanism for essentiallythe length of the first elongated hollow housing. The top side of thefirst elongated hollow housing has an elongated opening for essentiallythe length of the first elongated hollow housing. The elongated openingis surmounted by a vaulted, sealed covering. There is a power and drivemeans for the rotatable screw in and a first fill chamber surmounting afirst control value. There is a second fill chamber located beneath thefirst control valve, and a second control valve surmounting the secondfill chamber.

There is a metering means. The metering means is comprised of a secondelongated hollow housing having a top side. The second elongated hollowhousing contains therein a metering screw for essentially the length ofthe second elongated hollow housing. The top of the second elongatedhollow housing has an elongated opening for essentially the length ofthe second elongated hollow housing, the elongated opening is alsosurmounted by a vaulted, sealed covering, and there is a power and drivemeans for the metering screw of.

There is a reactor, the reactor comprises a third elongated hollow tube.The third elongated hollow tube has a near end and a distal end and atop side and is capped at the near end. The third elongated hollow tubehas a feed screw located in it for essentially the length of the thirdelongated hollow tube, and the third elongated hollow tube hassurmounted on it, a catalyst feed vessel, on the top side, near the nearend. The catalyst feed vessel has an upper valve and a lower valve andthere is a power and drive means for the feed screw of the reactor.

The system has a solids collection means located at the distal end ofthe third elongated hollow tube and a gas and liquid collection meanslocated at the distal end of the reactor.

Finally, the system has a means of providing a negative pressure to thesecond fill chamber, the metering means, the catalyst feeding vessel,and the reactor and a means of heating the second fill chamber, themetering means, the catalyst feeding vessel, and the reactor.

In another embodiment of this invention, there is a process forobtaining carbon-based products from hydrocarbons, using the systemdescribed just Supra, the process comprising providing a feed hopper, afeed conveyor having an elongated hollow housing having an elongatedopening therein that is surmounted by a vaulted, sealed covering, afirst fill chamber with a first control valve in an open position, asecond fill chamber, a second control valve in a closed position, ametering means having an elongated hollow housing having an elongatedopening therein that is surmounted by a vaulted, sealed covering, areactor comprising an elongated hollow housing having an elongatedopening therein that is surmounted by a vaulted, sealed covering and anentry port and an exit port, a catalyst feed vessel having a firstcontrol valve in an open position and a second control valve in a closedposition, a solids collection means, a gas and liquid collection means,a means of providing a negative pressure for the second fill chamber,metering means, catalyst feeding vessel, and reactor; a means of heatingthe second fill chamber, the metering means, the catalyst feedingvessel, and the reactor, and feeding a predetermined amount ofhydrocarbons into the feed hopper.

A negative pressure is provided on the second fill chamber, the meteringmeans, the catalyst feed vessel and the reactor and a predeterminedamount of hydrocarbons are fed into the first fill chamber and the firstcontrol valve is closed.

The second control valve is opened and allows the contents of the firstfill chamber to enter into the second fill chamber and the secondcontrol valve is then closed.

The reactor is then heated and the lower control valve of the catalystfill vessel is closed, and the upper control valve of the catalyst fillvessel is opened, and a predetermined amount of catalyst is introducedinto the catalyst fill vessel and the upper control valve is closed.

Thereafter, the lower control valve of the catalyst fill vessel isopened and the catalyst is allowed to enter the heated reactor. Thecontents of the second fill chamber are metered into the entry port ofthe reactor and the contents allowed to move through the reactor at apredetermined rate by the use of the rotatable screw, wherein thehydrocarbons react under the influence of the catalyst and providevolatile and solid carbon-based products.

The solid carbon-based products are allowed to separate and move fromthe volatile carbon-based products by gravity, to the solids collectionmeans through the exit port of the reactor, and the volatilecarbon-based products are allowed to move to the gas and liquidcollection means through the exit port of the reactor.

Yet another embodiment of this invention are the novel components of thesystem, for example, the reactor. The reactor comprises an elongatedhollow tube having a near end and a distal end that is capped at thenear end. The elongated hollow tube contains a rotatable screw having alength essentially equal to the length of the elongated hollow tube. Theelongated hollow tube has an opening through the top surface the openinghaving a length essentially equal to the length of the elongated hollowtube and the opening is covered and sealed by a vaulted cover.

The elongated hollow tube has a loading port near the near end, and anunloading port near the distal end. The elongated hollow tube hassurmounted near the near end, a catalyst fill vessel, the vessel havingan upper and a lower valve.

The elongated hollow tube has a means for heating the elongated hollowtube for essentially the entire length of it and the elongated hollowtube has the capability of holding a negative pressure.

Another embodiment consisting of novel components is the conveyor. Theconveyor comprises an elongated hollow tube having a near end and adistal end and a top surface. The conveyor contains a rotatable screw init having a length essentially equal to the length of the conveyor andthe elongated hollow tube has an opening through the top surface, theopening having a length essentially equal to the length of the elongatedhollow tube. The opening is covered and sealed by a vaulted cover.

Another embodiment of this invention is a novel carbon black that isproduced by the process of this invention.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a non-scale view in perspective of the system of thisinvention.

FIG. 2 is a cross sectional end view of the fee conveyor through lineA-A of FIG. 1.

FIG. 3 is a cross sectional end view of the metering means through lineB-B of FIG. 1.

FIG. 4 is a cross sectional end view of the reactor through line C-C ofFIG. 1.

FIG. 5 is a view in perspective of the feeding end of the system.

FIG. 6 is a view in perspective of the exiting end of the system.

FIG. 7 is a view in perspective of the solids collection means.

DETAILED DESCRIPTION OF THE INVENTION

Turning now to FIG. 1, which is a non-scale view of a large portion ofthe system of this invention, there shown a feed hopper 2, a feedconveyor 3, consisting of an elongated tube 4 containing a rotatablescrew 5 (FIG. 2), a first fill chamber 6, a second fill chamber 7, afirst control valve 8, a second control valve 9, a metering means thatconsists of an elongated hollow housing 10, a top side 11 of theelongated hollow housing 10, a rotatable screw 12 (FIG. 3) and anelongated opening 13 (FIG. 3), a vaulted, sealed covering 31 over theelongated opening 13, a power and drive means 14 for the rotatable screw5 of the feed conveyor 3, a power and drive means 15 for the rotatablescrew 12, a reactor 16 comprised of an elongated hollow housing 17,containing a rotatable screw 18 (FIG. 4), an elongated opening 19 (FIG.4) in the top side 20 of the elongated hollow housing 17, a vaulted,sealed covering 21 (FIG. 4) along the elongated hollow housing 17 andcovering the elongated opening 19, a catalyst feed vessel 22, having anear end 23 and a distal end 24, and having an upper valve 25 and alower valve 26, a power an drive means 27 for the rotatable screw 18 forthe reactor 16, a solids collection means 28, located at the distal end30 of the elongated hollow housing 17, a gas and liquid collection means29 located at the distal end 30 of the elongated hollow housing 17, thedetails of the collection means 28 and 29 being set forth below indetail infra.

Turning now to FIG. 5, wherein there is shown a view in perspective ofthe feeding end of the system showing the feed hopper 2, at the base 32of the conveyor 3. The feed hopper 2 is constructed such that it willhold water in its base 33. The water is used occasionally to enhance thereaction of the waste products in the reactor 16. For example, if rubbertires are the waste product, then water is used at the rate of from zeroto 50% by weight of the tire feed to the feed hopper 2. It is known bythe inventors herein that the higher the vacuum, the higher thetemperature, and with no water, the conversion is mainly to gases andliquids, while lower vacuum, lower temperature with water usuallyresults in a preponderance of carbon black.

The conveyor 3 is constructed of an elongated hollow tube 4 thatcontains a rotating screw 5 that collects the waste from the bottom 33of the feed hopper 2 and moves it up the elongated hollow tube 4 anddumps the waste into the first fill chamber 6. The elongated hollow tube4 is capped at its base end 32 by a sealed cap 36 and the top end of theelongated hollow tube 4 is also capped and sealed by a cap 37.

The bottom of the feed hopper 2 is open to allow the particles to bepicked up by the rotating screw 5 and moved to the first fill chamber 6,along with whatever water the particles pick up while resident in thefeed hopper 2. The rotatable screw 5 is powered and driven by a motor14, and preferred for this invention is a rate of rotation that willback fill the first fill chamber 6 and the second fill chamber 7 suchthat the feed can be moved by the metering system at the rate of up to10,000 pounds of waste per hour of operation. If tires are used by wayof example, the tire particles or chips should have a size that is 2inches square or less, and smaller particles are preferred, it beingnoted that shredded tires do not have a thickness much beyond about ½inch. Particles having a size smaller than 2 inches square enhances thereactivity of the particles when they enter the reactor 16. This systemis also useful for wastes such as plastics, carpet, wood chips, andother bio waste.

Surmounted on the top of the first fill chamber 6 is a first controlvalve 8 that is closed initially. The first fill chamber 8 is surmountedon a second fill chamber 7, and surmounted on the second fill chamber 7,and between the two chambers, is a second control valve 9. In operation,the first control valve 8 is open, and the second control valve 9 isclosed, and a vacuum is applied to the system from the distal end 30 ofthe reactor 16. With continuous application of negative pressure, thefirst fill chamber 6 is filled with a predetermined amount of wastematerial and the first control valve 8 is then closed. The secondcontrol valve 9 is then opened and the waste material is allowed to flowinto the second fill chamber, and then the second control valve 9 isclosed.

The first fill chamber 6 can contain a vibrating level indicator (notshown) that levels the materials that is fed to the first fill chamber6. This vibrating level indicator is positioned in the first fillchamber 6 at an angle of from zero to 45° from the vertical such thatdepending on the waste material, the waste material is leveled in thechamber by the vibration before it is moved into the second fill chamber7. The vibrating level indicator can have a high and a low levelindicator as well.

The feed is picked up by a rotating screw 12 (FIG. 3) and the rotatingscrew 12 is moved up through the elongated hollow tube 10 (FIG. 3) ofthe metering means 40 to eventually empty into the reactor 16 at thenear end 34 of the reactor 16. The elongated hollow tube 10 is cappedand sealed at its base by a cap 38 and at its top by a cap 39.

Unlike the conveyor elongated hollow tube 4, the elongated hollow tube10 of the metering means 40 has an elongated opening 13 in the top side11 (FIG. 3) that is capped and sealed with a vaulted, sealed covering31. Generally, since the material of construction for the elongatedhollow tubes is steel, the vaulted, sealed covering 31 is welded to thetop side 11 as is shown in FIG. 4 as 41. However, any means of sealingthis covering to the elongated hollow tube is acceptable.

The purpose of the vaulted covering 31 is to allow for the wastematerial to be moved along in the elongated hollow tube 10 withoutbinding on the rotatable screw 12 and jamming the rotatable screw 12.

When the waste material reaches the top 42 of the elongated hollow tube,it falls by gravity into the near end of the elongated hollow tube 17 ofthe reactor 16 where it is picked up by a rotatable screw 18 (FIG. 4).

Prior to the emptying of the waste material into the reactor 16, thereactor 16 is subjected to the catalyst for the reaction. This isaccomplished by mounting a catalyst feed vessel 22 near the near end 42of the elongated hollow tube 17. The catalyst feed vessel 22 opensdirectly into the reactor 16 and the catalyst loading is controlled bythe control valves 25 and 26. The reactor is heated to at least atemperature of 300° F. and preferred for this invention, the reactor 16is preheated to about 800° F. The upper control valve 25 is then openedand the bottom control valve 26 is closed. A predetermined amount ofcatalyst is loaded into the catalyst feed vessel 22 and the top valve 25is closed and the bottom control valve 26 is opened. The catalyst feedsby gravity, but is assisted by the negative pressure that is drawn onthe reactor 16.

This aspect of the invention is very important, as the catalyst must beadded to the preheated reactor 16 before any of the waste material isfed into the reactor 16. In this manner, it is believed that thecatalyst, as a very fine powder, coats the interior surface of theelongated hollow tube 17 and also the surfaces of the rotating screw 18.

If the catalyst is added in this fashion, it maintains as a coat on theinterior surface of the reactor 16 and the rotatable screw 18 and beavailable for all additional waste material that is fed into thereactor. If the catalyst is added in this manner, according to thisinvention, then no additional catalyst has to be added to the reactor 16for additional batches of waste material fed to the reactor 16. As longas the temperature of the reactor 16 is maintained in excess of 300° F.,batch after batch of waste material can be added to the reactor 16without having to add additional catalyst. This is a novel feature ofthis invention. If the temperature drops below about 300° F., then thecatalyst must be renewed for any additional waste material fed to thereactor and it must be carried out according to the protocol set forthabove for the invention.

After the catalyst has been added, the waste material from 40 is addedto the reactor 16 and the rotating screw moves the waste material alongthe elongated hollow tube 17 as it reacts and converts to the desirableproducts.

With reference to FIG. 6, which is an enlarged view of the distal ½ ofthe reactor 16, with the catalyst feed vessel 22 noted for purposes ofaligning the Figure with that of FIG. 5, it will be noted that theelongated hollow tube 17 has a vaulted, sealed covering 21 and that itis sealed by welds 41. The purpose of this vaulted, sealed covering 21is the same as for that in the metering means 40 and in addition, it isa means of preventing the rotatable screw 18 from scraping the catalystfrom the interior surface of the elongated hollow tube 17.

The elongated hollow tube 17 is heated for its entire length andmaintained in the range of about 400° F. and 1600° F. for the durationof the operation. Also, the second fill chamber 7, the metering means40, and the reactor 16 must all be under negative pressure. For purposesof this invention, the negative pressure can range from about 0.5 mm Hgto about 26 mm Hg, and the preferred ranges is from about 19 to 22 mmHg. The system of this invention can be equipped with standard equipmentsuch as temperature indictors, pressure indicators, load quantityindicators, and the like. Likewise, this system can be equipped andmonitored using computers for feeding, conveying heating, non-pressuringand pressuring, and the like.

The pitch of the rotatable screws in this system have a pitch of from 6to 12 inches per linear foot and preferred is 8 to 10 inches per linearfoot and most preferred is 8 inches per linear foot.

The reactor 16 is provided with a heating means that is preferred to beelectric band heaters. Also useful are heating mantles that areconfigured to the outside surface of the reactor 16. The reactor 16 canalso be provided with a cooling means which can be for example, coolingcoils around the outside surface of the reactor, or the cooling can beinternal cooling, such as through the rotatable screws, or it can be acombination of them. The heating system can also be by way of naturalgas or some other similar means. The total length of the reactor 16depends on the throughput desired in the system.

During the movement of the reacting materials from the near end 42 ofthe reactor 16 to the distal end of the reactor 30, the materialsbreakdown into various substituents ranging from volatile gases to oils,to organic compounds, to solids comprised mainly of carbon black. At thedistal end 30 of the reactor, the solids are separated from themainstream by gravity and drop down a hollow tube 43 into a solidsconveyor 44.

The volatile gases, and liquids from the reaction are conveyed out ofthe reactor via an exit port 45 and conveyance line 46 to a gas andliquid collection station 47. The gas and liquid collection station iscomposed of compressors, pipelines and various other equipment tocollect and separate the gases and liquids and convey them to variousstorage facilities. All of such equipment is known in the art and isstandard in the industry and is not shown in detail herein.

The solids collection system is essentially known in the art and isstandard in the industry. Turning to FIG. 7, which is an enlargedversion of the solids collection system of the invention, it consists ofthe solids conveyor 44 from the reactor 16 (not shown) to a magneticseparator 48 where any magnetically attracted metal is extracted andfunneled by a chute 49 into a collection bin 50. The solids are thenmoved to a collection bin 51 and a pneumatic conveyor 52 propels thesolids to a storage bin 53. From there, the solids are bagged or boxedthrough the means 54.

The catalysts for this process are alumino silicates in their variousforms such as mullites, zeolites, montmorillonites, and the like.

The carbon black produced by this process is novel in that it is carbonblack with a small amount of material on the surface that gives thecarbon black some unusual properties.

1. A process for obtaining carbon-based products from hydrocarbons, theprocess comprising: (A) providing a feed hopper; a feed conveyor havingan elongated hollow housing having an elongated opening therein that issurmounted by a vaulted, sealed covering; a first fill chamber with afirst control valve in an open position; a second fill chamber with asecond control valve in a closed position; a metering means having anelongated hollow housing having an elongated opening therein that issurmounted by a vaulted, sealed covering; a reactor comprising anelongated hollow housing having an elongated opening therein that issurmounted by a vaulted, sealed covering, a rotatable screw, an entryport and an exit port; a catalyst feed vessel having an upper controlvalve in an open position and a lower control valve in a closedposition; a solids collection means; a gas and liquid collection means;a means of providing a negative pressure for the second fill chamber,the metering means, the catalyst feed vessel, and the reactor; and ameans of heating the second fill chamber, the metering means, thecatalyst feed vessel, and the reactor; (B) feeding a predeterminedamount of hydrocarbons into the feed hopper; (C) providing a negativepressure on the second fill chamber, the metering means, the catalystfeed vessel and the reactor by the use of the means of providing anegative pressure; (D) feeding a predetermined amount of hydrocarbonsfrom the feed hopper into the first fill chamber by the use of the feedconveyor and closing the first control valve; (E) opening the secondcontrol valve and allowing the contents of the first fill chamber toenter into the second fill chamber and closing the second control valve;(F) heating the reactor using the means of heating; (G) introducing apredetermined amount of catalyst into the catalyst feed vessel andclosing the upper control valve; (H) opening the lower control valve ofthe catalyst feed vessel and allowing the catalyst to enter the heatedreactor; (I) metering the contents of the second fill chamber into theentry port of the catalyst containing heated reactor by the use of themetering means and allowing the contents to move through the reactor ata predetermined rate by the use of the rotatable screw, wherein thehydrocarbons react under the influence of the catalyst and providevolatile and solid carbon-based products; and (J) allowing the solidcarbon-based products to separate and move from the volatilecarbon-based products by gravity to the solids collection means throughthe exit port of the reactor, and allowing the volatile carbon-basedproducts to move to the gas and liquid collection means through the exitport of the reactor.
 2. The process as claimed in claim 1 wherein thehydrocarbons are continuously fed to the reactor, and the temperature inthe reactor does not decrease below about 300° F.
 3. The process asclaimed in claim 1 wherein there is additionally water present in thefeed hopper and the amount of water is up to 50% by weight based on theweight of the water and the hydrocarbons.
 4. The process as claimed inclaim 1 wherein the temperature for the process is in the range of 300°F. to 1600° F.
 5. The process as claimed in claim 1 wherein thetemperature for the process is in the range of 800° F. to 1200° F. 6.The process as claimed in claim 1 wherein the catalyst is selected fromthe group consisting of mullites, zeolites, and montmorillinite.
 7. Theprocess as claimed in claim 6 wherein the catalyst is aluminosilicate.8. The process as claimed in claim 7 wherein the aluminosilicate iszeolite.
 9. The process as claimed in claim 1 wherein the hydrocarbonsare particulate tire material.
 10. The process as claimed in claim 9wherein the particulates are 2 inches or less in size.
 11. The processas claimed in claim 1 wherein the hydrocarbons are waste hydrocarbons.